CN101519306A - Method for preparing high curie temperature leadless PTCR ceramic - Google Patents

Method for preparing high curie temperature leadless PTCR ceramic Download PDF

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CN101519306A
CN101519306A CN200910046521A CN200910046521A CN101519306A CN 101519306 A CN101519306 A CN 101519306A CN 200910046521 A CN200910046521 A CN 200910046521A CN 200910046521 A CN200910046521 A CN 200910046521A CN 101519306 A CN101519306 A CN 101519306A
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ptcr
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朱兴文
马季
姜文中
周晓
张芳
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a method for preparing high curie temperature leadless PTCR (positive temperature coefficient of resistor) ceramic sintered in atmosphere, which belongs to the technical field of processes for preparing electronic ceramic materials. The chemical molecular formula of the PTCR ceramic is a triple system of x(Bi1/2Na1/2)TiO3-yCaTiO3-(1-x-y)BaTiO3, wherein x is between 0.002 and 0.08, and y is between 0.03 and 0.30; besides, the PTCR ceramic is added with a 0.4 to 0.8 mol percent of semi-guided agent Y2O3, 0.03 to 0.12 mol percent of modifier MnO2, and 0.5 to 2.5 mol percent of sintering auxiliary agent SiO2; each material is weighed according to the molecular mol ratio of the chemical molecular formula, an additive is added to the materials to obtain a mixed batch, then a small amount of deionized water is added to the mixed batch, and the mixture is put into a ball mill to perform ball milling, wherein the weight ratio of the materials to balls to water is 1:2.5:1.5, and the ball milling time is between 24 and 72 hours; then the materials are taken out of the ball mill and are dried, polyvinyl alcohol is added to the dried materials to perform granulation, and the granules are pressed into round pieces at a pressure of 10 MPa; and the round pieces are sintered at a temperature of between 1,270 and 1,350 DEG C in the atmosphere to obtain the leadless PTCR ceramic in the end.

Description

The preparation method of high curie temperature leadless PTCR pottery
Technical field
The present invention relates to a kind of under air atmosphere the preparation method of agglomerating high curie temperature leadless PTCR (PTCR) pottery, belong to piezoelectric ceramics material preparation process technical field.
Background technology
Ferroelectric BaTiO 3Curie temperature Tc be 120 ℃, the Tc of PTCR material can pass through SrTiO 3Or PbTiO 3With BaTiO 3Solid solution is regulated.Present widely used high curie point PTCR pottery all adopts BaTiO 3-PbTiO 3System, Tc is high more, and the lead content in the material is many more.The air-conditioning heating PTCR element of consumption maximum, Curie temperature is about 250 ℃, and the content of PbO surpasses 30wt% in the element.From the angle of environmental protection, Pb is harmful to human body and environment.Therefore, researching and developing non-lead is that the PTCR material has significance to national economy and social development.
The unleaded research of PTCR material starts from the end of the eighties in last century, with ferroelectric (Na, Bi) TiO 3(being called for short BNT) and BaTiO 3Solid solution obtains (Ba, Bi, Na) TiO 3It is high-temp PTC R material.NBT is a kind of relaxation type ferroelectrics with complex perovskite structure, and its Curie temperature is 320 ℃, receives much attention as leadless piezoelectric material material.Studies show that, replace PbTiO with NBT 3When preparing the PTCR material, when the NBT solid solution capacity was 1.5mol%, the Curie temperature of material can reach 150 ℃.With (Na, Bi) TiO 3The increase of solid solution capacity, the room temperature resistivity of material sharply rises to insulation.And at nonoxidizing atmosphere such as N 2Or under reducing atmosphere sintering, even BNT content reaches 30mol%, the resistivity of PTCR material still can reach the practicability requirement.But need the sintering manufacture method of atmosphere protection to increase the technology cost.The present invention will be at BNT-BaTiO 3High-content is introduced ternary---CaTiO on the basis of two component system PTCR material 3, to suppress free Na among the BNT +And Bi 3+The toxic action of ion pair PTC effect improves the performance of agglomerating stupalith under the atmosphere.
PTCR is the abbreviation of English Positive Temperature Coefficient of Resistance, and its Chinese translation is a posistor.
Summary of the invention
The object of the present invention is to provide a kind of under air atmosphere the preparation method of agglomerating high-curie temperature (Tc〉130 ℃) lead-free PTCR pottery.
A kind of preparation method of high curie temperature leadless PTCR pottery is characterized in that having following preparation process and step:
A. press molecule mol ratio Bi 2O 3: Na 2O:TiO 2=0.5:0.5:1.0 and CaCO 3: the ratio of TiO2=1.0:1.0 takes by weighing above-mentioned analytically pure raw material; CaCO 3Purity count 97～99% by its weight percent; Bi 2O 3, Na 2O and TiO 2Purity be 99.5～99.89%;
B. be medium with agate ball and alcohol, by expecting: the part by weight of ball, alcohol=1:2.5:1.5 is with above-mentioned Bi 2O 3, Na 2O, TiO 2Compound ball milling 24～48 hours, oven dry back solid state reaction 1～4 hour under 920～980 ℃ of temperature obtains (Bi 1/2Na 1/2) TiO 3Powder; Same quadrat method is with above-mentioned CaCO 3And TiO 2Compound ball milling 24～48 hours, oven dry back solid state reaction 1～4 hour under 1150～1210 ℃ of temperature obtains CaTiO 3Powder; In addition, be ready to existing commercially available BaTiO 3Raw material, its purity are 99.9%;
C. press chemical molecular formula x (Bi 1/2Na 1/2) TiO 3-yCaTiO 3-(1-x-y) BaTiO 3Three-part system carries out weigh batching; X=0.002～0.08 wherein, y=0.03～0.30; The Y that adds semiconductor agent 0.4～0.8mol% in addition 2O 3, the MnO of properties-correcting agent 0.03～0.12mol% 2And the SiO of sintering aid 0.5～2.5mol% 2To add small amount of deionized water in the above-mentioned mixed batch, be put in and carry out ball milling in the ball mill, wherein expect: ball: water=1:2.5:1.5 (weight ratio), the ball milling time is 24～72 hours; Discharging is dried then, and the concentration of oven dry back adding 8wt% is that the polyvinyl alcohol of 10wt% carries out granulation, is pressed into the disk of φ 10 * 2.0mm with the pressure of 10MPa;
D. the above-mentioned disk that suppresses is put in and carries out sintering under the air atmosphere, sintering temperature is 1270～1350 ℃, and keeps under this temperature 10～60 minutes, makes its abundant sintering and realizes solid state reaction; The sample that sinters makes metallization with the coating of Ag-Zn slurry after surface grinding, finally obtain the high curie temperature leadless PTCR ceramics sample.
Make the PTCR pottery by the inventive method and can reach following performance: room temperature resistivity is 9～20 * 10 4Ω cm, Curie temperature Tc=130～170 ℃, liftdrag is 1 * 10 2～5 * 10 4, nonlinear factor α is 8～25%.
Embodiment
After now specific embodiments of the invention further being described in.
Embodiment one: press x (Bi 1/2Na 1/2) TiO 3-0.03CaTiO 3-(0.97-x) BaTiO 3+ 0.65atom%Y 2O 3+ 0.05atom%MnO 2The SiO of+2.0atom% 2(being abbreviated as BNCBTO3, wherein x=0.002-0.06mol) molecular formula is formed, and converses the quality of required each powder, accurately weighing then, and weighing quality such as following table:
Table 1 allocation sheet one (unit: g)
Numbering BNT BaTiO 3 CaTiO 3 Y 2O 3 MnO 2 SiO 2
BNCBT03-00 0 226.20 4.0783 0.7339 0.0435 1.2017
BNCBT03-02 0.4246 225.73 4.0783 0.7389 0.0435 1.2017
BNCBT03-04 0.8493 225.26 4.0783 0.7339 0.0435 1.2017
BNCBT03-06 1.2740 224.80 4.0783 0.7389 0.0435 1.2017
BNCBT03-08 1.6986 224.33 4.0783 0.7339 0.0435 1.2017
BNCBT03-10 2.1233 223.86 4.0783 0.7389 0.0435 1.2017
Ball milling in the deionized water (material: ball: water=1:2.5: 1.5) 24-72 hour, add PVA (concentration 10wt%) granulation of 8wt% after the oven dry, suppress the disk of Φ 10 * 2.0mm with the pressure of 10MPa.The disk of being suppressed is incubated 10-60 minute sintering under 1270-1350 ℃ in air.Metallize with the Ag-Zn slurry after grinding in the surface of sintered sample.With the temperature rise rate heating ceramic sample of 1 ℃/min, test its resistance-temperature profile, the gained result is as shown in table 2:
The relation of table 2 PTCR ceramics sample performance and BNT content
Figure A200910046521D00051
Embodiment two: press x (Bi 1/2Na 1/2) TiO 3-0.09CaTiO 3-(0.91-x) BaTiO 3+ 0.65atom%Y 2O 3+ 0.05atom%MnO 2The SiO of+2.0atom% 2(being abbreviated as BNCBT09, wherein x=0.002-0.06mol) molecular formula is formed, and converses the quality of required each powder, accurately weighing then, and weighing quality such as following table:
Table 3 allocation sheet two (units: g)
Numbering BNT BaTiO 3 CaTiO 3 Y 2O 3 MnO 2 SiO 2
BNCBT09-00 0 212.10 12.3249 0.7339 0.0435 1.2017
BNCBT09-02 0.4246 211.74 12.3249 0.7389 0.0435 1.2017
BNCBT09-04 0.8493 211.27 12.3249 0.7339 0.0435 1.2017
BNCBT09-06 1.2740 210.81 12.3249 0.7389 0.0435 1.2017
BNCBT09-08 1.6986 210.34 12.3249 0.7339 0.0435 1.2017
BNCBT09-10 2.1233 209.87 12.3249 0.7389 0.0435 1.2017
BNCBT09-12 2.5479 209.41 12.3249 0.7339 0.0435 1.2017
BNCBT09-15 3.1849 208.70 12.3249 0.7389 0.0435 1.2017
BNCBT09-20 4.2466 207.54 12.3249 0.7339 0.0435 1.2017
BNCBT09-30 6.3699 205.21 12.3249 0.7389 0.0435 1.2017
BNCBT09-40 8.4932 202.88 12.3249 0.7339 0.0435 1.2017
BNCBT09-50 10.6164 200.55 12.3249 0.7389 0.0435 1.2017
BNCBT09-60 12.7397 198.21 12.3249 0.7389 0.0435 1.2017
Ball milling in the deionized water (material: ball: water=1:2.5:1.5) 24-72 hour, add PVA (concentration 10wt%) granulation of 8wt% after the oven dry, suppress the disk of Φ 10 * 2.0mm with the pressure of 10MPa.The disk of being suppressed is incubated 10-60 minute sintering under 1270-1350 ℃ in air.Metallize with the Ag-Zn slurry after grinding in the surface of sintered sample.With the temperature rise rate heating ceramic sample of 1 ℃/min, test its resistance-temperature profile, the gained result is as shown in table 4:
The relation of table 4 PTCR ceramics sample performance and BNT content
Figure A200910046521D00061
Embodiment three: press x (Bi 1/2Na 1/2) TiO 3-0.15CaTiO 3-(0.85-x) BaTiO 3+ 0.65atom%Y 2O 3+ 0.05atom%MnO 2The SiO of+2.0atom% 2(being abbreviated as BNCBT15, wherein x=0.002-0.06mol) molecular formula is formed, and converses the quality of required each powder, accurately weighing then, and weighing quality such as following table:
Table 5 allocation sheet three (units: g)
Numbering BNT BaTiO 3 CaTiO 3 Y 2O 3 MnO 2 SiO 2
BNCBT15-0 0 198.21 20.3148 0.7339 0.0435 1.2017
BNCBT15-02 0.4246 197.75 20.3148 0.7389 0.0435 1.2017
BNCBT15-04 0.8493 197.28 20.3148 0.7339 0.0435 1.2017
BNCBT15-06 1.2740 196.81 20.3148 0.7389 0.0435 1.2017
BNCBT15-08 1.6986 196.35 20.3148 0.7339 0.0435 1.2017
BNCBT15-10 2.1233 195.88 20.3148 0.7389 0.0435 1.2017
BNCBT15-12 2.5479 195.42 20.3148 0.7339 0.0435 1.2017
BNCBT15-15 3.1849 194.72 20.3148 0.7389 0.0435 1.2017
BNCBT15-20 4.2466 193.55 20.3148 0.7339 0.0435 1.2017
BNCBT15-30 6.3699 191.22 20.3148 0.7389 0.0435 1.2017
BNCBT15-40 8.4932 188.89 20.3148 0.7339 0.0435 1.2017
BNCBT15-50 10.6164 186.55 20.3148 0.7389 0.0435 1.2017
BNCBT15-60 12.7397 184.22 20.3148 0.7389 0.0435 1.2017
Ball milling in the deionized water (material: ball: water=1:2.5:1.5) 24-72 hour, add PVA (concentration 10wt%) granulation of 8wt% after the oven dry, suppress the disk of Φ 10 * 2.0mm with the pressure of 10MPa.The disk of being suppressed is incubated 10-60 minute sintering under 1270-1350 ℃ in air.Metallize with the Ag-Zn slurry after grinding in the surface of sintered sample.With the temperature rise rate heating ceramic sample of 1 ℃/min, test its resistance-temperature profile, the gained result is as shown in table 6:
The relation of table 6 PTCR ceramics sample performance and BNT content
Figure A200910046521D00071
Embodiment four: press x (Bi 1/2Na 1/2) TiO 3-0.20CaTiO 3-(0.80-x) BaTiO 3+ 0.65atom%Y 2O 3+ 0.05atom%MnO 2The SiO of+2.0atom% 2(being abbreviated as BNCBT15, wherein x=0.002-0.06mol) molecular formula is formed, and converses the quality of required each powder, accurately weighing then, and weighing quality such as following table:
Table 7 allocation sheet four (units: g)
Numbering BNT BaTiO 3 CaTiO 3 Y 2O 3 MnO 2 SiO 2
BNCBT20-0 0 186.55 27.1886 0.7339 0.0435 1.2017
BNCBT20-02 0.4246 186.09 27.1886 0.7389 0.0435 1.2017
BNCBT20-06 1.2740 185.15 27.1886 0.7389 0.0435 1.2017
BNCBT20-08 1.6986 184.69 27.1886 0.7339 0.0435 1.2017
BNCBT20-10 2.1233 184.22 27.1886 0.7389 0.0435 1.2017
BNCBT20-15 3.1849 183.06 27.1886 0.7389 0.0435 1.2017
BNCBT20-20 4.2466 181.89 27.1886 0.7339 0.0435 1.2017
BNCBT20-30 6.3699 179.56 27.1886 0.7389 0.0435 1.2017
BNCBT20-40 8.4932 177.23 27.1886 0.7339 0.0435 1.2017
BNCBT20-50 10.6164 174.89 27.1886 0.7389 0.0435 1.2017
BNCBT20-60 12.7397 172.56 27.1886 0.7389 0.0435 1.2017
BNCBT20-70 14.8630 170.23 27.1886 0.7389 0.0435 1.2017
Ball milling in the deionized water (material: ball: water=1:2.5:1.5) 24-72 hour, add PVA (concentration 10wt%) granulation of 8wt% after the oven dry, suppress the disk of Φ 10 * 2.0mm with the pressure of 10MPa.The disk of being suppressed is incubated 10-60 minute sintering under 1270-1350 ℃ in air.Metallize with the Ag-Zn slurry after grinding in the surface of sintered sample.With the temperature rise rate heating ceramic sample of 1 ℃/min, test its resistance-temperature profile, the gained result is as shown in table 8:
The relation of table 8 PTCR ceramics sample performance and BNT content
Figure A200910046521D00081
Figure A200910046521D00091
Embodiment five: press x (Bi 1/2Na 1/2) TiO 3-0.27CaTiO 3-(0.73-x) BaTiO 3+ 0.65atom%Y 2O 3+ 0.05atom%MnO 2The SiO of+2.0atom% 2(being abbreviated as BNCBT15, wherein x=0.002-0.06mol) molecular formula is formed, and converses the quality of required each powder, accurately weighing then, and weighing quality such as following table:
Table 9 allocation sheet five (units: g)
Numbering BNT BaTiO 3 CaTiO 3 Y 2O 3 MnO 2 SiO 2
BNCBT27-0 0 170.23 36.7047 0.7339 0.0435 1.2017
BNCBT27-02 0.4246 169.76 36.7047 0.7389 0.0435 1.2017
BNCBT27-04 0.8493 169.30 36.7047 0.7339 0.0435 1.2017
BNCBT27-06 1.2740 168.83 36.7047 0.7389 0.0435 1.2017
BNCBT27-10 2.1233 167.90 36.7047 0.7389 0.0435 1.2017
BNCBT27-12 2.5479 167.43 36.7047 0.7339 0.0435 1.2017
BNCBT27-15 3.1849 166.73 36.7047 0.7389 0.0435 1.2017
BNCBT27-20 4.2466 165.57 36.7047 0.7339 0.0435 1.2017
BNCBT27-30 6.3699 163.23 36.7047 0.7389 0.0435 1.2017
BNCBT27-40 8.4932 160.60 36.7047 0.7339 0.0435 1.2017
BNCBT27-50 10.6164 158.57 36.7047 0.7389 0.0435 1.2017
BNCBT27-60 12.7397 156.24 36.7047 0.7389 0.0435 1.2017
Ball milling in the deionized water (material: ball: water=1:2.5:1.5) 24-72 hour, add PVA (concentration 10wt%) granulation of 8wt% after the oven dry, suppress the disk of Φ 10 * 2.0mm with the pressure of 10MPa.The disk of being suppressed is incubated 10-60 minute sintering under 1270-1350 ℃ in air.Metallize with the Ag-Zn slurry after grinding in the surface of sintered sample.With the temperature rise rate heating ceramic sample of 1 ℃/min, test its resistance-temperature profile, the gained result is as shown in table 10:
The relation of table 10 PTCR ceramics sample performance and BNT content
Figure A200910046521D00101

Claims (1)

1, a kind of preparation method of high curie temperature leadless PTCR pottery is characterized in that having following preparation process and step:
A. press molecule mol ratio Bi 2O 3: Na 2O:TiO 2=0.5:0.5:1.0 and CaCO 3: TiO 2The ratio of=1.0:1.0 takes by weighing above-mentioned analytically pure raw material; CaCO 3Purity count 97～99% by its weight percent; Bi 2O 3, Na 2O and TiO 2Purity be 99.5～99.89%;
B. be medium with agate ball and alcohol, by expecting: the part by weight of ball, alcohol=1:2.5:1.5 is with above-mentioned Bi 2O 3, Na 2O, TiO 2Compound ball milling 24～48 hours, oven dry back solid state reaction 1～4 hour under 920～980 ℃ of temperature obtains (Bi 1/2Na 1/2) TiO 3Powder; Same quadrat method is with above-mentioned CaCO 3And TiO 2Compound ball milling 24～48 hours, oven dry back solid state reaction 1～4 hour under 1150～1210 ℃ of temperature obtains CaTiO 3Powder; In addition, be ready to existing commercially available BaTiO 3Raw material, its purity are 99.9%;
C. press chemical molecular formula x (Bi 1/2Na 1/2) TiO 3-yCaTiO 3-(1-x-y) BaTiO 3Three-part system carries out weigh batching; X=0.002～0.08 wherein, y=0.03～0.30; The Y that adds semiconductor agent 0.4～0.8mol% in addition 2O 3, the MnO of properties-correcting agent 0.03～0.12mol% 2And the SiO of sintering aid 0.5～2.5mol% 2To add small amount of deionized water in the above-mentioned mixed batch, be put in and carry out ball milling in the ball mill, wherein expect: ball: water=1:2.5:1.5 (weight ratio), the ball milling time is 24～72 hours; Discharging is dried then, and the concentration of oven dry back adding 8wt% is that the polyvinyl alcohol of 10wt% carries out granulation, is pressed into the disk of φ 10 * 2.0mm with the pressure of 10MPa;
D. the above-mentioned disk that suppresses is put in and carries out sintering under the air atmosphere, sintering temperature is 1270～1350 ℃, and keeps under this temperature 10～60 minutes, makes its abundant sintering and realizes solid state reaction; The sample that sinters makes metallization with the coating of Ag-Zn slurry after surface grinding, finally obtain the high curie temperature leadless PTCR ceramics sample.
CN200910046521A 2009-02-24 2009-02-24 Method for preparing high curie temperature leadless PTCR ceramic Pending CN101519306A (en)

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Cited By (8)

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CN102976747A (en) * 2012-12-04 2013-03-20 广西新未来信息产业股份有限公司 Lithium niobate doped barium titanate based positive temperature coefficient resistance material and preparation method thereof
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CN104557024A (en) * 2014-12-18 2015-04-29 天津大学 High-Curie-temperature lead-free barium-titanate-base PTCR (positive temperature coefficient of resistance) ceramic material, and preparation and application thereof
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Publication number Priority date Publication date Assignee Title
CN102976747A (en) * 2012-12-04 2013-03-20 广西新未来信息产业股份有限公司 Lithium niobate doped barium titanate based positive temperature coefficient resistance material and preparation method thereof
CN103342556A (en) * 2013-06-24 2013-10-09 湖北大学 Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material
CN103342556B (en) * 2013-06-24 2014-12-03 湖北大学 Preparation method of two-phase low-temperature co-sintered temperature stable dielectric ceramic material
CN104557024A (en) * 2014-12-18 2015-04-29 天津大学 High-Curie-temperature lead-free barium-titanate-base PTCR (positive temperature coefficient of resistance) ceramic material, and preparation and application thereof
CN104538134A (en) * 2014-12-26 2015-04-22 常熟联茂电子科技有限公司 Thermistor slurry
CN106145933A (en) * 2016-06-12 2016-11-23 上海大学 A kind of high-curie temperature (Tc > 190 DEG C) low lead PTCR ceramic material preparation method
CN106278250A (en) * 2016-08-29 2017-01-04 上海大学 A kind of preparation method of unleaded semistor pottery
CN113860728A (en) * 2021-11-24 2021-12-31 中国地质大学（北京） SiO based on ordered interface combination2-CaCO3-TiO2Composite ceramic opacifier and preparation method thereof
CN113860728B (en) * 2021-11-24 2023-05-09 中国地质大学（北京） SiO based on ordered interface combination 2 -CaCO 3 -TiO 2 Composite ceramic opacifier and preparation method thereof
CN114520114A (en) * 2022-02-24 2022-05-20 电子科技大学 High-temperature-stability sodium bismuth titanate-based medium energy storage ceramic material and preparation method thereof

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